Prosper barriers



1 UNITED STA rRosP s BriRRIERE, or PARIS, FRANCE.

PATENT OFFICE.

"LUMINOIUS "IMVIVATYEVRIAL FOR'INCANDESCENT GAS-LIGHTING.

SPECIFIGATIONiforming eat: Letters Patent No. 567,571, dated September 8, 1896. Application filed November 13, 1895. Serial No- 568,836. i (No specimens.) Patented in IranceMareh 28, 1895, No. 246,163.

To all whom it may concern:

Beitknown that I, PROSPER BAR IERE, a citizen of the Republic of France, residing in Paris, France, have invented a Novel Luminous and Radiating Body for Incandescent Lighting and Methodsof Making the Same, (for which I have obtained French Patent No. 246,163, dated March 28, 1895,) of'which the following is a specification.

Incandescentv gas-lighting, which consists in suspending fireproof luminous substances within the flame of a Bunsen burner, has been realized hitherto in several ways. 'The illuminating properties possessed by various metallic oxids, such as zirconium, lanthanum, yttrium, thorium, and magnesium, have suggested the ideaof making these oxids serviceable as luminous bodies.

The numerous experiments which I have made have enabled me to discover and to satisfy myself of the presence of a novel illumihating-body in a special ore of asandy na ture,obtainable at difierentplaces and known as monazite sand. This body, to which I have given the name lucium, has properties dififerent from those possessed by the substances used hitherto, and as to the constituency of which new body I am unable to statedefinitely at present whether it consists in a new element, a mixture of old' elements, or a mixture of a new element and old elements, but which I obtain in the manner hereinafter described. The ore is a river sand rich in small rubies. The monazite sands, obtained from difierent places, have all of them given me lucium; but I have specially eXperimented With'those coming from North Car0- lina and. from Brazil.

The following is an example of an analysis made on a sample of this substance: (SiO silica, 69.7 per cent.; (F 0 phosphoric acid, six per cent. (Fe O iron oxid, 1 92'per cent. (A1 0 alumina, fifteen per cent.; cerium, lanthanum, didymium, about2l3 percent; moisture,2.05percent.; lime, magnesia, and others, about two per cent.; lucium, 1.80 per cent. Luciumcnters into the composition of the ores-named in the proportion of from 1.5 to six per cent, according to the samples dealt with.

The composition indicated above neoessi tates special methods of treatment having for theirobject to eliminate any harmful substances. The purity of this body is the main condition'upon which a satisfactory yieldde- 5 pends.

The'ore, on having been porphyrized, is slowly melted in suitable furnaces, with an addition of carbonate of sodium, in the proportion of one part of ore for every two parts of carbonate. This operation, which it takes, about three hours to complete, is intended to convert the oxide into insoluble carbonates. This conversion is, of course, made at the melting temperature of carbonate of sodium.

After cooling, the powdered'mass is lixi-viated. V I

By means of decantation the elimination of the'silicates and phosphates of sodium is proceeded withn'The carbonates separated 7?;

by water are then submitted to the action of sulfuricacid, the surplus of which is eliminated by slow calcination.' The sulfates are dissolved in cold water, and as the sulfate of lime is rather insoluble, thisdisposes of a large proportioniof lime present, and the solution is then precipitated by means of ammonia. The precipitate on beingwashed is dissolved in hydrochloric acid,

care being takento properlyneutralize it by means of ammonia. To the neutralized solution oxalic acid ora solution of some soluble oxalateis added, and most of the ironand alumina remain in th'esolution and are separated by filtration. lates, among which are to be found the oxalates-of lucium and of the rarer earthscerium, lanthanum, didymium, thorium:- f are converted into sulfates by addition of sulfuric acid, heating, and partial calcina- 9o 7 tion in a muffle-furnace to eliminate thesurplus not in combination. The sulfates obtained are then pulverized and put in coldwater at a temperature of +4! centigrade,-in

small quantities, until a solution as nearly 5 saturated. as possible is obtained. The magnesia present will probably remain in solution as oxalate of magnesia and thus be separated. The solution obtained is then precipitated by ammonia, whereby traces-of r00 magnesia and salts of lime remain in the liquid and are eliminated, while. by filtering,

The insoluble oxaa gelatinous precipitate of oxids of lucium and of the rarer earths-cerium, lanthanum, thorium-is kept on the filter. This precipitate, washed with water, is once more treated by means of sulfuric acid. The surplus of the sulfuric acid is neutralized by sodium. To the solution crystals of sulfate of sodium are added until saturation- --Aft6P six hours of digestion at ordinary temperature cerium, lanthanum, didymium,.in a state of insoluble double sulfates, are separated, while thorium, lucium, and yttrium remain in the filtered liquid. The precipitate is washed in a saturated solution of sulfate of sodium. The prime liquid and the waters from the washing are put together and'treated by ammonia, which precipitates lucium, thorium, and yttrium, the only rarer earths remaining.

The precipitate by ammonia, gathered on a filter and washed, is treated, as previously, by sulfuric acid, the surplus of which is neutralized by potassium, and to the solution Now the principal operation of the process begins. It consists in precipitating lucium by means of a warm concel'itrated solution of hyposulfite of sodium in the hot hydrochloric solution. Lucium alone is precipitated. \Vhen it has been in ebullition for some time, I filter and wash with water to eliminate the hyposulfite of sodium. The body obtained contains by way of impurities small quantities of yttrite earths, principally ytterbium. ltonly remains after this to effect a. most thorough washing of the insoluble hyposulfitc precipitate thus obtained, using After w'asln cold water for the purpose. ing follows solution in hydrochloric acid. If there are any other impurities,'-they may be removed by any of the well-known methods. The hydrates are then precipitated from the hydrochloric-acid solution by addition of ammonia, and after precipitation the body is energetically washed with distilled water.

I obtain lucium, the characteristic properties of which I will now describe.

Compounds of Lucium.

The anhydrous oxid: The compound obtained as hereinbefore mentioned,-and after calcination, is .the anhydrous oxid of lucium.- It appears as a white mass, slightly grayish, insoluble in acids, even concentrated, and in 'ebullition, except in concentrated sulfuric cium are soluble in water.

acid, which dissolves it whcnwarm, converting it into sulfate.

The hydrated oxid: This oxid is prepared in precipitating the solution of sulfate of luci um by ammonia. It is a white gelatinous precipitate, easily soluble in diluted and even in weak acids. On account of this property salts of lucium may be easily obtained. \Vhen calcined, itbecomes anhydrous. The sulfate: It is prepared as hereinbefore mentioned. It is easily soluble in water, by means of which it can form several hydrates. The solution of this salt saturated with sulfate of potassium or sodium does not yield any insoluble double sulfates.

The nitrate: This salt is obtained by dissolving hydrate of lucium in nitric acid. Its solution, when evaporated until of a syrupy consistency, becomes converted into a crystalline mass formed by small white rosy crystals. This salt is very soluble in water. \Vhen calcined, it leaves anhydrous oxid of lucium.

The carbonate is ob taincd by precipitating a salt of luci um soluble in carbonate of sodium. It is a white powder insoluble in water.

The acetate and chlorid are white rosy salt-s susceptible of crystallization, and obtained by dissolving hydrate of luci um in hydrochloric or acetic acid.

The oxalate is prepared by adding oxalic acid to an aqueous solution of a salt of lucium until saturation. It deposits a white crystalline powder, insoluble, which is oxalate of lucium. \Vhen calcined, it yields anhydrous oxid of lucium.

Lucium is different from the other rarer earths known, ona-ccount of the following reactions: Sulfate, nitrate, and chloridof lu- Oxalate of 111 ciu in is insoluble, and this distinguishes it from glucinium' Lucium does not yield, like cerium, lanthanum, and didymium, any double sulfate insoluble with sulfate of potassium. It does not form, as thorium does, any double sulfate insolublewith sulfate of potassium. It is precipitated by liyposulfite of sodium. Yttrium, ytterbium, and the salts of cerium are not precipitated by that hyposulfit-e. Lastly, its atomic weight1ucium, -1-distinguishes it fromthe rarer earths known.

Lucium maybe applied to the manufacture of skeletons or mantles for incandescent gaslighting in any of the methods adapted for the manufacture of such articles with other oxids. For instance, a fabric of suitable fibrous materialmay be impregnated with a solution of the oxid of lucium, and after drying the textile material may be burned out,

; leaving a skeleton or mantle ready for us.

I claim as my invention- 1'. As a new article of manufacture, a luminous material for lighting by incandescence, consisting essentially of lucium, de-

rived from monazite sands and hving the characteristics hereinbefore described.

2. The mode herein described of obtaining too 567,571 I r s sands by fusion with carbonate of sodium,

, separating the silicate and phosphate of sodium, attacking the insoluble carbonates by sulfuric acid, dissolving the sulfates in cold water, causing precipitation. by ammonia, dissolving the precipitates in hydrochloric acid, causing precipitation by oxalic acid, conversion of V oxalates into sulfates, redissolving these by sulfuric acid, causing precipitation by hyposulfite of sodirun and dissolving in hydrochloric acid, substantially as described.

In testimony whereof I have signed. my name to this specification in the presence of two subscribing Witnesses.

PROSPER BARRIER'E.

Witnesses LEON FRA-NCKERD, CLYDE SHROPSHIRE. 

